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Concentrated sample introduction method for realizing trace components for chromatograph

A technology for trace components and chromatograph, which is applied in the field of chromatograph to realize the concentration and sampling of trace components, and can solve the problems of inability to analyze solid samples, broadening of sampling bands, and inability to concentrate trace components, etc. Wide range of samples and the effect of improving detection sensitivity

Inactive Publication Date: 2005-06-29
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of headspace sampling technology is that it cannot concentrate trace components in gas samples, it is only suitable for the concentration of volatile components in solid or liquid; The highest concentration efficiency can only reach the thermal equilibrium value
Analytical sensitivity and quantitative accuracy are directly affected due to incomplete desorption of concentrated trace components
Thermal desorption technology is very suitable for the concentrated analysis of trace components in gas samples, but it is generally not suitable for the concentrated treatment of liquid samples, because the adsorbed liquid will generate a large amount of gas when heated and desorbed, which will cause sample injection Severe broadening of the band; in addition, in order to completely desorb the adsorbed components, when the non-equilibrium thermal desorption method is used, the continuous flow of the desorption airflow will also cause the broadening of the sample band and affect the chromatographic Column separation efficiency and detection sensitivity
If the equilibrium desorption method is used in thermal desorption, the disadvantages of headspace sampling technology cannot be avoided.
Cool on-column sampling technology is very effective for the analysis of trace components in liquid samples, but its scope of application is limited and cannot be used for analysis of solid samples
Pyrolysis sampling technology can be directly used to analyze trace volatile components in solid samples, but it also has the weakness of headspace and thermal desorption sampling technology

Method used

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  • Concentrated sample introduction method for realizing trace components for chromatograph
  • Concentrated sample introduction method for realizing trace components for chromatograph
  • Concentrated sample introduction method for realizing trace components for chromatograph

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] operating conditions

[0020] Gas chromatography column: HP-5, 30m×0.32mm×0.25μm

[0021] Detector: FID, temperature 250°C

[0022] Column temperature: programmed temperature increase at 35°C, hold for 0min, then increase temperature to 300°C at 15°C / min

[0023] Injector: split injection, split ratio 1:1, temperature 250°C

[0024] Sample: Particulate matter in the exhaust gas of internal combustion engines (contains a large amount of carbon and trace amounts of saturated hydrocarbons, aromatic hydrocarbons and other substances that pollute the environment)

[0025] Analysis by conventional headspace technology: first heat treatment of glass fiber filter paper at 600°C for 5 hours, and then capture particulate matter in exhaust gas of internal combustion engine. Put the filter paper with trapped particles into the headspace balance device, keep the temperature at 280°C for 30 minutes, purge and trap the balance gas, and directly inject samples for analysis. No volat...

Embodiment 2

[0028] operating conditions

[0029] Gas chromatography column: HP-5, 12m×0.22mm×0.25μm

[0030] Detector: MS (mass spectrometry), temperature 185°C

[0031] Column temperature: program temperature rise to 70°C for 2 minutes, then increase temperature to 280°C at 25°C / min

[0032] Injector: Split injection, split ratio 1:20, temperature 250°C

[0033] Sample: Natural Rubber and Butadiene Rubber Blend

[0034]Put a small amount of powdered rubber sample into the reactor and carry out the cracking reaction at a high temperature of 800 ° C for 5 minutes, and the gas components generated by the cracking reaction are continuously sent to the secondary concentration device. At this time, the temperature of the secondary concentration device is -30°C, and the reaction gas produced by cracking is continuously concentrated. After the cracking reaction is completed, the temperature of the secondary concentration device is increased to 280°C, and the concentrated reaction gas compone...

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Abstract

This invention relates to a condensation sample-in method to realize the trace content of the chromatogram, which belongs to the improvement technique of the chromatogram. It is to set the initial and second condensation devices in the entrance of the color spectrum column and to set heating and second condensation devices in the entrance of the color entrance sending the components into the color spectrum column; to set the reactor and second condensation device in the entrance of the color spectrum entrance; after the reaction to improve the temperature of the second condensation device to send the components into the color spectrum column.

Description

technical field [0001] The invention relates to a chromatographic instrument to realize a concentrated sample injection method of trace components, which belongs to the improved technology of chromatographic instrument sample injection. Background technique [0002] How to achieve high-sensitivity detection of trace substances and effective separation of complex samples are two major problems in chromatography research. In order to improve the detection of trace components, it is often necessary to pre-treat the sample so that the analyzed sample components are pre-concentrated before analysis. The instrumental methods for pre-concentration mainly include headspace sampling technology, thermal desorption technology, cold on-column sampling technology and thermal cracking sampling technology. The disadvantage of headspace sampling technology is that it cannot concentrate trace components in gas samples, it is only suitable for the concentration of volatile components in soli...

Claims

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Application Information

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IPC IPC(8): G01N30/04G01N30/08
Inventor 范国梁宋崇林宋威龚彩荣
Owner TIANJIN UNIV
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